微波消解-电感耦合等离子体发射光谱法测定岩石和矿物中的钼
Determination of Molybdenum in Rock and Mineral Samples by Microwave Digestion-Inductively Coupled Plasma-Atomic Emission Spectrometry
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摘要: 用盐酸-氢氟酸-硝酸微波消解对样品进行前处理,电感耦合等离子体发射光谱法测定岩石和矿物中的钼,选择202.03 nm为样品分析谱线,优化了微波消解的实验条件,可消解多个样品,减少了碱熔分解样品方法引入的基体干扰,避免了极谱法中汞对人体的伤害。用不同类型国家一级标准物质分析验证,测定结果与标准值吻合。方法精密度(RSD,n=8)小于2.0%,加标回收率为96.4%~101.3%,方法检出限为0.0005%。该方法适用于岩石和矿物中钼的测定,制样速度快,操作简便安全,样品重现性好,能满足简单、快速、批量分析的要求。
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关键词:
- 钼 /
- 岩石 /
- 矿物 /
- 电感耦合等离子体发射光谱法 /
- 微波消解
Abstract: Molybdenum in rock and mineral samples were dissolved by HCl-HF-HNO3 with micro-wave digestion, and measured by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The experimental conditions for microwave digestion were optimized, for example, select 202.03 nm spectral line for sample analysis, run multi samples simultaneously and reduce the matrix interference by alkali fusion. The damages to the human body were avoided as not using mercury compared with method of polarography. The reliability of the method has been tested by kinds of national standard and results were in agreement with certified value. The recoveries of the method are 96.4%-101.3% with precision of less than 2.0% (RSD, n=8). The detection limit of the method was 0.0005% for molybdenum. The method had been applied to the determination of molybdenum in rock and mineral samples with satisfactory results. The method holds the advantages of low detection limit, good reproducibility, high sensitivity, high efficiency, simple operation and suitable for the routine sample analysis.-
Keywords:
- molybdenum /
- rocks /
- minerals /
- inductively /
- coupled /
- plasma-atomic /
- emission /
- spectrometry /
- microwave
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周永义,古学新,钱可萍.微波消解技术及其在分析化学中的应用[J].冶金分析,2004,24(2):68-70. 白锁柱,今海燕,周秀清.蒙药额日敦乌日勒微量元素的微波消解ICP-AES测定[J].光谱实验室,2007,24(2):262-264. 周淼,徐烨,迂君,薛峰.ICP-AES法测定滑子蘑中的Cd、Cu、Pb和Zn[J].分析试验室,2008,27(6):101-104. 付志红,谢明勇,章志明,郭岚.ICP-AES法测定车前子中无机元素[J].光谱学与光谱分析,2004,24(6):737-740. 康清蓉,罗财红.ICP-AES法测定饮用水中的Cu、Mn、Pb、Cd、Zn[J].光谱实验室,2002,19(5):611-613. 韩立新,李冉.ICP-AES法测定茶叶、茶水中的矿物质和微量元素[J].光谱学与光谱分析,2002,22(2):304. 王松君,常平.ICP-AES法同时测定人法、血液、唾液、牙齿中的多种元素[J].光谱学与光谱分析,1992,12(1):79-82. 常平,王松君,王飞.ICP-AES法测定林蛙组织中多种微量元素方法研究[J].光谱学与光谱分析,2003,23(3):556-559. 王松君,常平,孙春华,苏维娜,管奕.ICP-AES法测定蚂蚁粉中多种微量元素[J].光谱实验室,2002,19(1):131-133. 吕杰.ICP-AES法同时测定饮用水中Pb、As等11种金属元素[J].光谱学与光谱分析,2003,23(4):779-784. 方奕文,郝志峰,宋一兵,孙长勇,余坚,余林.ICP-AES法测定六氟磷酸锂中21种杂质元素[J].光谱学与光谱分析,2005,25(5):280. 李文龙,荆淼,陈军辉,陈登云,王小如.微波消解-ICP-AES测定40种中药材中的5种有毒元素[J].分析试验室,2008,27(2):6-9. 岩石矿物分析编写组.岩石矿物分析(第一分册)[M].3版.北京: 地质出版社,1991:540-551. 邓勃.应用原子吸收与原子荧光光谱分析[M].2版.北京:化学工业出版社,2007:288-289. 张力民,刘敏,杨丽君.ICP-AES测定饮用水中微量钼[J].光谱实验室, 2007,24(5):860-862.
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